# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Ian Fairlamb'
_publ_contact_author_address     
;
Department of Chemistry
University of York
Heslington
York
YO10 5DD
UNITED KINGDOM
;

_publ_contact_author_email       IJSF1@YORK.AC.UK

_publ_section_title              
;A natural light induced regioselective
6pi-electrocyclisation / oxidative aromatisation reaction: Experimental
and theoretical insights
;
loop_
_publ_author_name
'Ian Fairlamb'
'Hao Dong.'
'Simon B. Duckett'
'Zhenyang Lin.'
'Benjamin E. Moulton'
;
C.T.O'Brien
;

# Attachment 'ijf0613m.cif'

data_ijf0613m
_database_code_depnum_ccdc_archive 'CCDC 624078'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 O3'
_chemical_formula_sum            'C22 H18 O3'
_chemical_formula_weight         330.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1515(8)
_cell_length_b                   10.0702(10)
_cell_length_c                   10.3368(10)
_cell_angle_alpha                71.999(2)
_cell_angle_beta                 80.438(2)
_cell_angle_gamma                71.163(2)
_cell_volume                     761.69(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2236
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             348
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.905
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_process_details   'SADABS v2.03;(Sheldrick)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7944
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         28.34
_reflns_number_total             3760
_reflns_number_gt                2875
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.0804P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3760
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.23201(17) 0.71494(14) 0.44141(13) 0.0206(3) Uani 1 1 d . . .
C2 C 0.16935(16) 0.60406(13) 0.54895(12) 0.0176(3) Uani 1 1 d . . .
C3 C 0.22769(16) 0.46058(13) 0.53924(12) 0.0179(3) Uani 1 1 d . . .
C4 C 0.34294(17) 0.42517(14) 0.42543(13) 0.0191(3) Uani 1 1 d . . .
H4 H 0.3825 0.3273 0.4197 0.023 Uiso 1 1 calc R . .
C5 C 0.39449(17) 0.52912(14) 0.32780(13) 0.0202(3) Uani 1 1 d . . .
C6 C 0.50781(19) 0.51459(15) 0.20127(14) 0.0251(3) Uani 1 1 d . . .
H6A H 0.5413 0.4132 0.1973 0.038 Uiso 1 1 calc R . .
H6B H 0.6123 0.5424 0.2017 0.038 Uiso 1 1 calc R . .
H6C H 0.4444 0.5786 0.1215 0.038 Uiso 1 1 calc R . .
C7 C 0.16687(16) 0.35141(13) 0.64203(13) 0.0179(3) Uani 1 1 d . . .
C8 C 0.05321(16) 0.38785(14) 0.74745(13) 0.0185(3) Uani 1 1 d . . .
C9 C -0.00932(16) 0.53281(13) 0.76142(12) 0.0182(3) Uani 1 1 d . . .
C10 C -0.12818(17) 0.56790(15) 0.87067(13) 0.0219(3) Uani 1 1 d . . .
H10 H -0.1667 0.4935 0.9381 0.026 Uiso 1 1 calc R . .
C11 C -0.18785(18) 0.70824(15) 0.87957(14) 0.0244(3) Uani 1 1 d . . .
H11 H -0.2674 0.7311 0.9533 0.029 Uiso 1 1 calc R . .
C12 C -0.13218(18) 0.81867(15) 0.78026(14) 0.0247(3) Uani 1 1 d . . .
H12 H -0.1751 0.9161 0.7872 0.030 Uiso 1 1 calc R . .
C13 C -0.01678(17) 0.78842(14) 0.67334(14) 0.0221(3) Uani 1 1 d . . .
H13 H 0.0194 0.8650 0.6072 0.027 Uiso 1 1 calc R . .
C14 C 0.04941(16) 0.64393(13) 0.66011(13) 0.0184(3) Uani 1 1 d . . .
C15 C 0.21271(17) 0.19201(13) 0.64808(12) 0.0183(3) Uani 1 1 d . . .
H15 H 0.1777 0.1784 0.5659 0.022 Uiso 1 1 calc R . .
C16 C 0.40287(17) 0.10298(13) 0.67672(12) 0.0189(3) Uani 1 1 d . . .
H18 H 0.4924 0.1467 0.6167 0.023 Uiso 1 1 calc R . .
C17 C 0.42186(18) -0.05425(14) 0.67675(13) 0.0219(3) Uani 1 1 d . . .
H17A H 0.5457 -0.1115 0.6716 0.026 Uiso 1 1 calc R . .
H17B H 0.3657 -0.0552 0.5993 0.026 Uiso 1 1 calc R . .
C18 C 0.32752(18) -0.11526(14) 0.81516(14) 0.0237(3) Uani 1 1 d . . .
H18B H 0.2336 -0.1510 0.8017 0.028 Uiso 1 1 calc R . .
H18A H 0.4099 -0.1956 0.8764 0.028 Uiso 1 1 calc R . .
C19 C 0.25359(17) 0.01771(14) 0.87237(13) 0.0212(3) Uani 1 1 d . . .
H19 H 0.2185 -0.0055 0.9723 0.025 Uiso 1 1 calc R . .
C20 C 0.10931(17) 0.12794(14) 0.78056(13) 0.0200(3) Uani 1 1 d . . .
H20 H 0.0311 0.0786 0.7614 0.024 Uiso 1 1 calc R . .
C21 C 0.00682(17) 0.25508(14) 0.83660(13) 0.0209(3) Uani 1 1 d . . .
C22 C 0.40241(17) 0.08839(14) 0.82881(13) 0.0204(3) Uani 1 1 d . . .
H22A H 0.3727 0.1838 0.8487 0.024 Uiso 1 1 calc R . .
H22B H 0.5128 0.0234 0.8681 0.024 Uiso 1 1 calc R . .
O1 O 0.34101(12) 0.67015(10) 0.33558(9) 0.0220(2) Uani 1 1 d . . .
O2 O 0.19856(13) 0.84297(10) 0.43188(10) 0.0296(3) Uani 1 1 d . . .
O3 O -0.09555(13) 0.24905(11) 0.93615(10) 0.0316(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0179(6) 0.0190(6) 0.0237(6) -0.0049(5) -0.0006(5) -0.0050(5)
C2 0.0172(6) 0.0167(6) 0.0182(6) -0.0031(5) -0.0031(5) -0.0048(5)
C3 0.0177(6) 0.0176(6) 0.0172(6) -0.0029(5) -0.0031(5) -0.0043(5)
C4 0.0213(6) 0.0167(6) 0.0183(6) -0.0047(5) -0.0003(5) -0.0047(5)
C5 0.0206(6) 0.0201(6) 0.0195(6) -0.0049(5) -0.0020(5) -0.0055(5)
C6 0.0294(7) 0.0245(7) 0.0200(6) -0.0046(5) 0.0035(5) -0.0097(6)
C7 0.0179(6) 0.0171(6) 0.0179(6) -0.0035(5) -0.0019(5) -0.0051(5)
C8 0.0178(6) 0.0184(6) 0.0186(6) -0.0040(5) -0.0020(5) -0.0051(5)
C9 0.0170(6) 0.0191(6) 0.0179(6) -0.0047(5) -0.0028(5) -0.0044(5)
C10 0.0203(6) 0.0247(7) 0.0197(6) -0.0060(5) -0.0005(5) -0.0056(5)
C11 0.0220(7) 0.0272(7) 0.0231(7) -0.0110(5) 0.0007(5) -0.0032(5)
C12 0.0257(7) 0.0197(6) 0.0292(7) -0.0110(5) -0.0025(6) -0.0029(5)
C13 0.0219(6) 0.0195(6) 0.0252(7) -0.0060(5) -0.0034(5) -0.0056(5)
C14 0.0173(6) 0.0184(6) 0.0191(6) -0.0050(5) -0.0033(5) -0.0039(5)
C15 0.0214(6) 0.0172(6) 0.0165(6) -0.0041(5) -0.0006(5) -0.0068(5)
C16 0.0207(6) 0.0173(6) 0.0179(6) -0.0044(5) 0.0002(5) -0.0055(5)
C17 0.0256(7) 0.0175(6) 0.0219(6) -0.0061(5) -0.0002(5) -0.0053(5)
C18 0.0275(7) 0.0178(6) 0.0240(7) -0.0043(5) 0.0010(5) -0.0071(5)
C19 0.0245(7) 0.0183(6) 0.0183(6) -0.0032(5) 0.0012(5) -0.0059(5)
C20 0.0209(6) 0.0186(6) 0.0209(6) -0.0039(5) 0.0008(5) -0.0089(5)
C21 0.0195(6) 0.0210(6) 0.0212(6) -0.0040(5) 0.0004(5) -0.0072(5)
C22 0.0219(6) 0.0196(6) 0.0192(6) -0.0063(5) -0.0018(5) -0.0043(5)
O1 0.0249(5) 0.0177(5) 0.0218(5) -0.0039(4) 0.0020(4) -0.0070(4)
O2 0.0324(6) 0.0172(5) 0.0353(6) -0.0059(4) 0.0059(5) -0.0074(4)
O3 0.0322(6) 0.0280(6) 0.0307(6) -0.0074(4) 0.0134(5) -0.0119(4)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.2041(15) . ?
C1 O1 1.3831(16) . ?
C1 C2 1.4683(18) . ?
C2 C3 1.3978(17) . ?
C2 C14 1.4477(18) . ?
C3 C7 1.4277(17) . ?
C3 C4 1.4386(17) . ?
C4 C5 1.3345(18) . ?
C4 H4 0.9500 . ?
C5 O1 1.3685(15) . ?
C5 C6 1.4883(18) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.3684(17) . ?
C7 C15 1.5095(17) . ?
C8 C9 1.4273(17) . ?
C8 C21 1.4930(18) . ?
C9 C10 1.4146(18) . ?
C9 C14 1.4258(17) . ?
C10 C11 1.3652(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.401(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.3700(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.4207(18) . ?
C13 H13 0.9500 . ?
C15 C16 1.5444(18) . ?
C15 C20 1.5568(17) . ?
C15 H15 1.0000 . ?
C16 C22 1.5326(17) . ?
C16 C17 1.5402(17) . ?
C16 H18 1.0000 . ?
C17 C18 1.5531(19) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.5349(18) . ?
C18 H18B 0.9900 . ?
C18 H18A 0.9900 . ?
C19 C22 1.5359(18) . ?
C19 C20 1.5469(18) . ?
C19 H19 1.0000 . ?
C20 C21 1.5099(19) . ?
C20 H20 1.0000 . ?
C21 O3 1.2115(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 114.61(11) . . ?
O2 C1 C2 128.03(12) . . ?
O1 C1 C2 117.34(11) . . ?
C3 C2 C14 121.62(11) . . ?
C3 C2 C1 117.90(11) . . ?
C14 C2 C1 120.48(11) . . ?
C2 C3 C7 118.76(11) . . ?
C2 C3 C4 120.31(11) . . ?
C7 C3 C4 120.90(11) . . ?
C5 C4 C3 120.31(12) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 O1 120.59(12) . . ?
C4 C5 C6 128.03(12) . . ?
O1 C5 C6 111.37(11) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C3 120.14(11) . . ?
C8 C7 C15 113.33(11) . . ?
C3 C7 C15 126.53(11) . . ?
C7 C8 C9 122.93(11) . . ?
C7 C8 C21 108.94(11) . . ?
C9 C8 C21 128.11(12) . . ?
C10 C9 C14 120.12(12) . . ?
C10 C9 C8 121.82(11) . . ?
C14 C9 C8 118.06(11) . . ?
C11 C10 C9 120.29(12) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.20(12) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 121.02(12) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.79(12) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 117.58(12) . . ?
C13 C14 C2 123.93(11) . . ?
C9 C14 C2 118.48(11) . . ?
C7 C15 C16 115.28(10) . . ?
C7 C15 C20 103.53(10) . . ?
C16 C15 C20 102.71(10) . . ?
C7 C15 H15 111.6 . . ?
C16 C15 H15 111.6 . . ?
C20 C15 H15 111.6 . . ?
C22 C16 C17 102.27(10) . . ?
C22 C16 C15 101.56(10) . . ?
C17 C16 C15 106.74(10) . . ?
C22 C16 H18 114.9 . . ?
C17 C16 H18 114.9 . . ?
C15 C16 H18 114.9 . . ?
C16 C17 C18 103.37(10) . . ?
C16 C17 H17A 111.1 . . ?
C18 C17 H17A 111.1 . . ?
C16 C17 H17B 111.1 . . ?
C18 C17 H17B 111.1 . . ?
H17A C17 H17B 109.1 . . ?
C19 C18 C17 102.97(10) . . ?
C19 C18 H18B 111.2 . . ?
C17 C18 H18B 111.2 . . ?
C19 C18 H18A 111.2 . . ?
C17 C18 H18A 111.2 . . ?
H18B C18 H18A 109.1 . . ?
C18 C19 C22 100.99(10) . . ?
C18 C19 C20 107.12(11) . . ?
C22 C19 C20 102.43(10) . . ?
C18 C19 H19 114.9 . . ?
C22 C19 H19 114.9 . . ?
C20 C19 H19 114.9 . . ?
C21 C20 C19 112.93(11) . . ?
C21 C20 C15 106.11(10) . . ?
C19 C20 C15 103.38(10) . . ?
C21 C20 H20 111.3 . . ?
C19 C20 H20 111.3 . . ?
C15 C20 H20 111.3 . . ?
O3 C21 C8 126.57(12) . . ?
O3 C21 C20 125.42(12) . . ?
C8 C21 C20 108.00(11) . . ?
C16 C22 C19 94.68(10) . . ?
C16 C22 H22A 112.8 . . ?
C19 C22 H22A 112.8 . . ?
C16 C22 H22B 112.8 . . ?
C19 C22 H22B 112.8 . . ?
H22A C22 H22B 110.2 . . ?
C5 O1 C1 123.52(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 -179.35(13) . . . . ?
O1 C1 C2 C3 1.77(18) . . . . ?
O2 C1 C2 C14 1.3(2) . . . . ?
O1 C1 C2 C14 -177.54(11) . . . . ?
C14 C2 C3 C7 -0.06(19) . . . . ?
C1 C2 C3 C7 -179.36(11) . . . . ?
C14 C2 C3 C4 178.19(11) . . . . ?
C1 C2 C3 C4 -1.12(18) . . . . ?
C2 C3 C4 C5 -0.33(19) . . . . ?
C7 C3 C4 C5 177.88(12) . . . . ?
C3 C4 C5 O1 1.10(19) . . . . ?
C3 C4 C5 C6 -177.92(13) . . . . ?
C2 C3 C7 C8 0.18(19) . . . . ?
C4 C3 C7 C8 -178.05(12) . . . . ?
C2 C3 C7 C15 179.06(11) . . . . ?
C4 C3 C7 C15 0.8(2) . . . . ?
C3 C7 C8 C9 -0.32(19) . . . . ?
C15 C7 C8 C9 -179.34(11) . . . . ?
C3 C7 C8 C21 178.10(11) . . . . ?
C15 C7 C8 C21 -0.92(15) . . . . ?
C7 C8 C9 C10 179.35(12) . . . . ?
C21 C8 C9 C10 1.2(2) . . . . ?
C7 C8 C9 C14 0.32(19) . . . . ?
C21 C8 C9 C14 -177.78(12) . . . . ?
C14 C9 C10 C11 0.23(19) . . . . ?
C8 C9 C10 C11 -178.78(12) . . . . ?
C9 C10 C11 C12 0.2(2) . . . . ?
C10 C11 C12 C13 -0.4(2) . . . . ?
C11 C12 C13 C14 0.1(2) . . . . ?
C12 C13 C14 C9 0.29(19) . . . . ?
C12 C13 C14 C2 178.97(12) . . . . ?
C10 C9 C14 C13 -0.47(18) . . . . ?
C8 C9 C14 C13 178.58(11) . . . . ?
C10 C9 C14 C2 -179.23(11) . . . . ?
C8 C9 C14 C2 -0.18(18) . . . . ?
C3 C2 C14 C13 -178.62(11) . . . . ?
C1 C2 C14 C13 0.7(2) . . . . ?
C3 C2 C14 C9 0.06(19) . . . . ?
C1 C2 C14 C9 179.35(11) . . . . ?
C8 C7 C15 C16 -112.33(12) . . . . ?
C3 C7 C15 C16 68.73(16) . . . . ?
C8 C7 C15 C20 -0.99(14) . . . . ?
C3 C7 C15 C20 -179.93(12) . . . . ?
C7 C15 C16 C22 73.96(12) . . . . ?
C20 C15 C16 C22 -37.87(12) . . . . ?
C7 C15 C16 C17 -179.30(10) . . . . ?
C20 C15 C16 C17 68.88(11) . . . . ?
C22 C16 C17 C18 31.39(13) . . . . ?
C15 C16 C17 C18 -74.84(12) . . . . ?
C16 C17 C18 C19 4.32(13) . . . . ?
C17 C18 C19 C22 -38.42(12) . . . . ?
C17 C18 C19 C20 68.40(13) . . . . ?
C18 C19 C20 C21 171.62(10) . . . . ?
C22 C19 C20 C21 -82.58(12) . . . . ?
C18 C19 C20 C15 -74.16(12) . . . . ?
C22 C19 C20 C15 31.64(12) . . . . ?
C7 C15 C20 C21 2.43(13) . . . . ?
C16 C15 C20 C21 122.73(11) . . . . ?
C7 C15 C20 C19 -116.62(11) . . . . ?
C16 C15 C20 C19 3.69(12) . . . . ?
C7 C8 C21 O3 -177.07(13) . . . . ?
C9 C8 C21 O3 1.3(2) . . . . ?
C7 C8 C21 C20 2.52(14) . . . . ?
C9 C8 C21 C20 -179.16(12) . . . . ?
C19 C20 C21 O3 -70.89(17) . . . . ?
C15 C20 C21 O3 176.55(13) . . . . ?
C19 C20 C21 C8 109.52(12) . . . . ?
C15 C20 C21 C8 -3.04(14) . . . . ?
C17 C16 C22 C19 -53.94(11) . . . . ?
C15 C16 C22 C19 56.26(11) . . . . ?
C18 C19 C22 C16 56.66(11) . . . . ?
C20 C19 C22 C16 -53.82(11) . . . . ?
C4 C5 O1 C1 -0.37(19) . . . . ?
C6 C5 O1 C1 178.80(11) . . . . ?
O2 C1 O1 C5 179.88(11) . . . . ?
C2 C1 O1 C5 -1.09(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.053